Nanoscale Synthesis and Characterization (NSC)
We design and study atomic-scale to meso-scale materials with implications for energy, the environment, and coherent information transfer and sensing.
The Nanoscale Synthesis and Characterization (NSC) group seeks to investigate and manipulate materials at the atomic, molecular, and mesoscopic scale to better understand and utilize their behavior and properties. Through this understanding and control, we aim to pave the way for breakthroughs in next-generation energy conversion technologies, materials synthesis, and quantum information science.
The NSC research comprises several key areas, including understanding of (1) electronic, mechanical, and optical response on the atomic and molecular scale, especially in low-dimensional materials, self-assembled systems, single-molecule and defect studies on surfaces, and molecular motors on surfaces and (2) structural organization, energy transduction, and dissipation on the mesoscopic scale. The latter includes nanoscale self-assembly and dynamics of nanoparticles in complex fluids.
Investigation of nanoscale phenomena often requires experimental approaches that extend beyond conventional techniques. To that end, NSC exploits highly advanced instrumentation, such as ultrahigh vacuum scanning probe microscopies (UHV SPM), single-particle laser spectroscopy, and novel approaches for hybrid, organic, and nanoparticle materials synthesis.
Research activities include:
- Low-dimensional materials synthesis and characterization
- Atomistic investigations of engineered surfaces, interfaces, and molecular self-assemblies
- Optical interactions and photo-physics on nanometer and atomic length scales
- Quantum information and sensing with dopants/defects near surfaces
- Hybrid nanoparticles and nanomaterials for energy applications
- AI-driven nanomaterial synthesis to enable unique nanomaterials for energy and environmental applications.
- Particle dynamics and energy dissipation in complex fluids under nonequilibrium conditions.
Key Capabilities
- UHV SPMs: Omicron VT-AFM/STM, Omicron Cryo SFM, Omicron LT-STM/q+AFM, Createc LT SPM, and Omicron UHV VT-AFM/q+/STM with optical access
- Synchrotron X-ray scanning tunneling microscopy at APS Sector 4 (XTIP)
- Ambient AFMs, including an Asylum Cypher S (bluedrive) and Bruker (Veeco) MultiMode 8
- Physical vapor deposition (Lesker CMS 18 and PVD 250)
- Magnetic property measurement system and physical property measurement system
- Colloidal chemistry and self-assembly techniques
- Rheo-SAXS-XPCS
- Lakeshore probe station
Group capabilities
Agilent Inductively Coupled Plasma Optical Emission spectroscopy (ICP-OES, Bldg 200)
Inductively Coupled Plasma Optical Emission Spectroscopy (ICP-OES or ICP-AES) is a technique that uses a plasma as a source and relies on optical emission for analysis. It is mainly used for liquid samples, which first need to be turned into an aerosol and then are injected into the plasma. Solid samples can be analyzed after acid digestion. The Agilent 5110 Synchronous Vertical Dual View (SVDV) ICP-OES is a high sensitive and versatile instrument, as the instrument captures the axial and radial views of the plasma in one measurement. Installed in 2018, the instrument became available for users in February 2021.
Asylum Cypher-S AFM (NST SOP 290)
The Asylum Cypher atomic force microscope (AFM) system provides routinely achievable high resolution, fast scanning capabilities and simple operation. Tapping mode is the primary method available for users, though other modes of operation and cantilever drive (such as bluedrive) are possible. These require further training and some experience of the user.
Cary 5000 UV-Vis-NIR (Building 200)
The Cary 5000 is a high-performance UV-Vis and NIR spectrophotometer with photometric performance in the 175–3300 nm range. Using a PbSmart detector, the Cary 5000 extends its NIR range to 3300 nm making it a powerful tool for materials science research. Installed in 2003, this instrument became available to users in Feb. 2021.
Differential scanning calorimetry, Mettler Toledo 823
DSC is capable of measuring thermal response of materials of both organic and inorganic composition. They can be used to identify the transitions between complex ordering phases as well as to determine the thermal stability of the sample at various temperatures. The analyzer has a refrigeration/heating system capable of maintaining sample temperature from −150°C to 700°C under inert gas. The instrument has high resolution, superior baseline precision, and reproducibility (<±25 ìW). The cell sensitivity is very high (~ 0.2 ìW detection) for sample of low volume (~ 1 mg).
DynaCool 14T PPMS
Quantum Design DynCool PPMS system with temperature range of 1.8 to 400 K, and magnetic field range +/- 14T. Options include Resistivity, Rotator, Electrical Transport (ETO), Vibrating Sample Magnetometry (VSM), and AC Susceptibility (ACMS II).
Lesker e-beam evaporator (PVD250)
Kurt Lesker Dual Chamber Sputtering-Electron-Beam Evaporation System. This tool, managed by the QEM Group, is housed in the clean room facility. It offers sputtering and e-beam evaporation capabilities with a wide range of deposition parameters by which polycrystalline and amorphous films of a wide group of materials can be deposited onto substrates up to 6 inches in diameter. A common load-lock assembly and robotic arm allows sample transfer from one system to the other without breaking vacuum. The addition of a 2nd e-beam gun during FY 2016 allows for the sequential evaporation of up to 10 different materials, thus increasing the efficiency and productivity of the tool, in addition to having the capability for co-evaporation of metals and alloys.
Lesker sputtering system (CMS18)
Kurt Lesker Dual Chamber Sputtering-Electron-Beam Evaporation System. This tool, managed by the QEM Group, is housed in the clean room facility. It offers sputtering and e-beam evaporation capabilities with a wide range of deposition parameters by which polycrystalline and amorphous films of a wide group of materials can be deposited onto substrates up to 6 inches in diameter. A common load-lock assembly and robotic arm allows sample transfer from one system to the other without breaking vacuum. The addition of a 2nd e-beam gun during FY 2016 allows for the sequential evaporation of up to 10 different materials, thus increasing the efficiency and productivity of the tool, in addition to having the capability for co-evaporation of metals and alloys.
Low temperature multimode scanning tunneling microscopy (LT-STM, Createc) (NST-SOP-196.2)
Createc 4K STM/AFM with thin film preparation and characterization facilities (441/pad #4). This instrument is available for atom manipulation and is capable of imaging both conducting and non-conducting samples at 4.8 K and 80 K substrate temperatures. The system also has the capability to apply an internal vertical magnetic field of up to 2.5 T. The STM/q+AFM setup allows simultaneous measurement of tunneling current and force signals, thereby enabling tunneling and force spectroscopy experiments at sub-atomic resolution. The STM/q+AFM scanner and the bath cryostat are housed in a UHV chamber that can be separated from the main UHV chamber via a gate valve. The main UHV chamber includes state-of-the-art UHV pumps and pressure monitoring instruments, an Omicron VT STM setup, an Omicron low-energy electron diffraction system, a Varian reflection high-energy electron diffraction (RHEED) system, an ion sputtering system, and a manipulator with XYZ translational and rotational stages. The sample temperature at the manipulator stage can be varied from 20 K to 2000 K using liquid helium cooling and e-beam and/or resistive heating. The chamber also has a standard load-lock system, and a fast entry load-lock system separated by gate valves.
Omicron LT-STM (SOP 303)
Atomic resolution low temperature scanning tunneling microscope (LT-STM) capable to cool down a sample to 5K. The microscope is attached to a sample preparation chamber. The system’s capable techniques: sample sputtering, sample annealing, physical vapor deposition (PVD), controlled gas dosing, temperature programmed desorption (TPD), atomic-scale imaging, scanning tunneling spectroscopy (STS).
Optical UHV VT STM/AFM (NST-SOP-126.9)
Omicron UHV VT AFM/STM with Optical Access
Quantum Design MPMS-XL
Quantum Design Magnetic Properties Measurement System (MPMS XL) is a high-sensitivity SQuID magnetometer system that provides vital information on the magnetic properties of high-temperature superconductors, biomagnetic systems, and magnetic nanoparticles and thin films at temperatures ranging from 1.9 K to 400 K. It is equipped with a 7-tesla High Uniformity magnet, the Reciprocating Sample Option with a DC measurement sensitivity of 1 x 10-8 emu, the 7-tesla AC Measurement System (M123) for measuring from 0.1 Hz to 1 kHz, and both horizontal and vertical sample rotators (M101D). The maximum sample size is 9 mm.
Quantum Design PPMS-9
Quantum Design Physical Properties Measurement System (PPMS-9) is a versatile system for characterizing materials properties at temperatures from 1.9 K to 400 K at magnetic fields up to 9 tesla (longitudinal field). This system features an open architecture that is designed to perform a variety of automated measurements but can also be adapted to a wide range of experiments requiring variable temperature and/or magnetic field. Many options are available, including DC resistivity with 12 connection points, an AC susceptibility/DC magnetization measurement option, an AC transport property measurement system, a high-resolution horizontal sample rotator with high-resolution computer- controlled stepper motor, and a heat capacity measurement system.
Rheo-XPCS
This is a capability jointly developed by a collaboration between CNM and APS. The instrument allows simultaneous measurement of rheological properties of complex fluids, structure measurement through in situ small angle x-ray scattering technique, and dynamics of structural evolution through x-ray photon correlation spectroscopy.
Rheometer, AntonPaar Physica MCR301
Anton Paar PHYSICA MCR301 Rheometer determines the viscosity and viscoelastic properties of a wide range of materials and is capable of examining their behavior under specific experimental conditions. With the use of an environmental control unit, the temperature-dependent viscoelastic properties also can be explored. The rheometer can perform a wide range of steady and dynamic tests in both controlled-stress and controlled-strain modes, with minimum torque of 0.1 mNm and a resolution of 0.001 mNm. The rheometer is permanently associated with the APS Sector 8 beamline for the shared APS/CNM Rheo-XPCS capability.
Scanning probe microscope, Veeco MultiMode 8 (NST-SOP-006.9)
Veeco NanoScope V Scanning Probe Microscope is capable of atomic force imaging in standard contact and tapping mode, with possible simultaneous collection of eight data channels. This instrument is also capable of torsional resonance imaging to obtain lateral force information, fluid imaging, variable-temperature (-35°C to 250°C) imaging in an inert atmosphere, and low-current STM. The microscope is situated on an active vibration isolation table within an acoustic chamber, thereby eliminating the vast majority of external noise.
SPM Tip Etching
Electrochemical etching of scanning probe tips
Synchrotron X-ray Scanning Tunneling Microscopy (B125)
A homebuilt synchrotron X-ray scanning tunneling microscope (SX-STM) equipped with a sample cleaning and preparation chamber. The microscope can be operated at room temperature under ultra-high vacuum environment. It can run both normal STM mode (without X-ray) and SX-STM mode (with X-ray).
Thermogravimetric analysis, Mettler Toledo 851
Thermogravimetry (TGA) is a technique that measures the change in weight of a sample as it is heated, cooled or held at constant temperature. Its main use is to characterize materials with regard to their composition. Application areas include plastics, elastomers and thermosets, mineral compounds, ceramics and nanomaterials. Main Features and benefits of the METTLER TOLEDO TGA/DSC 3+:
UHV Cryo SFM with 6T magnetic field, Omicron scanning tunneling microscope (NST-SOP-205)
Omicron 4K SPM (441/pad #2). This instrument is capable of imaging conducting samples at 4 K with an external field up to 6 Tesla. It includes two ultra-high-vacuum chambers equipped with basic surface preparation and analysis tools. A tip exchange mechanism and appropriate adapters allow the preparation of magnetic tips for spin- polarized STM. Vertical stability of below 10 pm can be achieved.
UV-Vis-NIR spectrometer, Perkin-Elmer Lambda 950
Perkin-Elmer Lamda 950 UV/Vis/NIR Spectrometer is a double-beam, double-monochromator ratio recording system with pre-aligned tungsten-halogen and deuterium lamps as sources. The wavelength is guaranteed to an accuracy of 0.05 nm from 175 to 3300 nm in the UV-Vis region, and to an accuracy of 0.2 nm in the NIR region. It has a photometric range of +/−8 in absorbance.
VT-UHV-atomic force microscope/scanning tunneling microscope (AFM/STM; Omicron VT-AFM XA) (NST-SOP-086.6)
Variable Temperature UHV Atomic Force and Scanning Tunneling Microscope (VT-AFM/STM) (440/B102). This is a commercial Omicron system capable of imaging insulating and conducting samples at temperatures between 50 K and 500 K. It includes two UHV chambers equipped with basic surface preparation and analysis tools. A tip exchange mechanism and appropriate adapters allow the preparation of magnetic tips for magnetic force microscopy and spin-polarized STM measurements. Vertical stability of below 20 pm has been achieved.
X-ray diffractometer (Bruker D2 Phaser XRD)
Bruker D2 Phaser Diffractometer with LYNXEYE Detector provides rapid X-ray characterization of polycrystalline samples. The D2 Phaser is equipped with a line detector that greatly decreases the data acquisition time while providing better signal-to-noise ratio than the scintillation detector on the D8 Discover system. The D2 Phaser reduces the demand for the high-resolution Bruker D8 Discover diffractometer while providing better-quality polycrystalline characterization in much less time.
X-ray diffractometer (Bruker D8 Discover, Eiger 2 R 500K detector)
Bruker D8 discover instrument is a cutting edge x-ray material structure characterization instrument, with application in both thin film and powder samples. The D8 DISCOVER with DAVINCI design increases ease-of-use with real-time component detection, plug-and-play functionality and fully integrated 2-dimensional XRD2 capabilities. These unique features allow the user to easily switch between all materials research X-ray diffraction applications, including reflectometry, high-resolution diffraction, grazing incidence diffraction (IP-GID), small angle X-ray scattering (SAXS), as well as residual stress and texture investigations. It has Im Cu source and Eiger 2R 500 area detector.
X-Ray diffractometer (Bruker D8 Discover, point detector, VANTEC-1 linear detector)
Bruker D8 Discover Diffractometer with Concentric Eulerian Cradle provides high-resolution four-circle X-ray characterization of bulk, powder, and thin-film samples. It is equipped with a Cu X-ray source and multiple optics and detector options. It is suitable for x-ray reflectivity, high-resolution XRD, reciprocal space mapping (RSM), grazing-incidence diffraction, Bragg- Brentano, rocking curves, texture, and stress characterization. The diffractometer is equipped with a VÅNTEC-1 detector to accelerate RSM measurements.